Distilling process



E. J. WINTER.

DISTILLING PROCESS.

APPLICATION FILEDJUNE I3. 1918.

Patented Sept. 5, 1922.

3 SHEETS-SHEET I.

E. J. WINTER msmuwe PROCESS.

APPLICATION FILED JUNE I3. I9I8.

1,427,885. PatentedSept. 5, 1922.

3 SHEETS SHEET 2.

l I 43 24 I E. J. WINTER.

DISTILLING PROCESS.

APPLICATION FILED JUNE 13. 1918.

Patented Sept. 5, 1922.

umrro STATES PATENT orrica.

nausea muons WINTER, or BALTIMORE, MARYLAND, assrcnoa To s. mnusramr. ALCOHOL 0a, A coaromrron or wasr vraemra.

DISTILLING raocnss.

Y Application filed June 13, 918. Serial in. 239,753.

To all whom it may: concern:

Be it knownthat I, Ennns'r JEROME WIN- TuR,'of Baltimore, in the State of Maryland,

Pr ess-a apt d t be used in d l butit 1135 lefrenoe especially to the distillation" of a ohol.

.he o ject of my n entionis p d a process by which distillates of a high deg e of pu ity and, s r ngth may b ta and specia ly to pr d a di t l g PIOQQSS n which eryhigh proof alcoho or a te alcohol, be obtained.

- A further ob'e tof my i P ide a pro es of the above character n whi h the d stil ates referred to y be readily obtained at a minim m costa with minimum amo nt of labor, th c rr sp n g apparatus b ng claimed my app i eon S.]N. 239,754.

Hitherto, in the distill'ation of alcohol, owing to the use of atmospheric pressures and columns, alcohol of a greater strength than 95.4% could not be obtained, for the,

reason that at atmospheric'pressures, when the strength of the alcohol being distilled or rectified has reached 95.4%, the va or produced. un er th s onditio s W 1 d have the same strength. Furthermore, in the said processes, if any attempt were made to apply vacuum to pan columns, this would be ineffective because of the fact that thecolumns would prevent the vacuum from acting to any great degree'below the first few pans at the top of the column connected with the vacuum pump, inasmuch as there are liquid seals between theseveral pans which gradually increase the head of liquid between the upper and lower portions of each column.

The object of my invention is, therefore, to "obviate the disadvantages inherent 1n previous methods provided O.r distill1ng alcohol, and particularly to provide a process in which a vacuum may be readily a plied, so that advantage may be taken of t e fact that under the influence of a" vacuum the vapors obtained from alcohol having a strength of 95.4% or higher contain even a nv n on i largenpercentage of alcohol than the liquid from which said vapors are derived.

Still another object of my'invention is to provide a'process of this nature in which a body of alcohol of increasing strength is brought into contact with a body of vapor,

also of increasing strength but which has a lower strength than the body of vapor that would be derived from and be in equilibrium with the portion" of said body of alcohol with which it would be in contact at any one time.

That is to say,.the object of my invention is particularly to provide a process of this kind in wh ch there is an advancing film of alcohol, having a progressively increasing strength toward 'its rearmost portion,

"tions, and the strength of the alcohol vapors at any given point bein less than. the strength of the vapor WlllCll would be in equilibrium with the liquid at'that point, but greater than the strength of the liquid itself, so thatas the current of vapor advances it will become richer in alcohol, while the current of liquid as it advances will become poorer in alcohol.

Another o'bfect of my invention is to bring about this action in a body of alcohol vapors obtained from an alcohol still, and to furthermore treat the weak alcohol. liquors thus obtained in a similar manner so as to bring up, their strength to the strength of the body of alcohol vapors originally treated, so that they may thereafter be united with a furthr quantity of the alcohol vapors from' the duce high proof alcohol.

Further objects of my invention will aptherewith in the accompanying drawings, in

same taken on line 44.

the same being optionally connected with a In the drawings, I have shown an alcohol still 1, carried upon any suitable framework 2, and which may be provided with a manhole 3, two glass windows 4 and 5 for viewing the progress of the distillation, a steam heating acket 6 provided with a steam inlet pipe 7, a valved feed pipe 8 for the inlet of weak alcohol, as for example 35% alcohol, the same being optionally connected with a supply tank 9, which may have a gauge 10, and a drain-pipe 11. A vapor outlet pipe 12 may be provided at the top of the still 1,

foam trap 13, having a return pipe 14 to said still. The vapor outlet pipe 12 may lead into a middle section 15 of a tubular rectifier 16, and may be at its extreme end an upwardly bent portion 17, which may pass through a diaphragm 18 extending across said middle section 15, which diaphragm 18 may be a plurality of holes 19 to receive the lowermost ends of a number of vertically arranged tubes 20 extending upwardly in said rectifier 16. The holes 19 are preferably somewhat larger than the external diameters of the tubes 20, so as to provide outlets for the alcohol or other vapors in a. downward direction through the diaphragm 18, in order to effectively distribute the alcohol vapors in the middle section 15 prior to the entry of the same into the lower ends of the tubes 20. Said tubes 20 may be held in place near their lower ends by means of a plate 21, through which they pass, and in which they may be tightly secured, said plate 21 being located at the upper end of the middle section 15, and being secured thereto,

as well as to an-upper rectifier section 22, by means of e. g. bolts 23. Said upper rectifier section 22 may be connected by means of valved pipe 24 and-pipe 25 to a preheater 26, which may be adapted to be supplied with steam by means of pipes 27 and 28. The preheater is designed to be used only when starting the operation of the apparatus, so as to provide in the upper section of the rectifier 22 the desired temperature from the beginning of the operation thereof. After the desired temperature has been reached, the preheater 26 will ordinarily be thrown out of operation by the closing of its valves, and thereafter a cooler 29 will ordinarily be. brought into operation, which cooler may be connected by pipes 30 and 31 to said upper section 22, said pipe 30 having therein a thermostat 30 and a circulating pump 30 which circulates a current of cooling water in the upper section 22. The cooler 29 may be supplied with cold water by means of pipes 32 and 33. At the upper end of the upper section 22, there may be a cover 34, havinga vapor outlet pipe 35 secured to the top thereof. Between the cover 34 and the upper section 22 there' may be a plate 35*, in which the upper ends of the tubes 20 may be secured, said late 35 being secured to the cover 34 and tiie upper section 22 by means of bolts 35. Any liquid that is condensed in the middle section of the rectifier 15 above the diaphragm 18 and the liquid that is condensed in the tubes 20 is received upon the upper surface of a plate 36, located at the bottom of the middle section l5,which plate 36 may have secured therein the upper ends of a number of tubes 37, that extend downwardly in a lower section 38, which may be secured to the plate 36 form of a film in the tubes the upper ends of said tubes may be provided with smaller L-shaped tubes 40. fitting therein and supported in place by e. g. brackets 41 and which may have upper horizontally-directed portions 42 to prevent the entry of the descending liquids into the same, while permitting the exit of the vapors ascending from the tubes 37.

Initially it is sometimes found desirable to supply a quantity of liquid into the middle section 15 without waiting for the ac: cumulation thereof from the upper section 22, and for this purpose the tube 8 used for supplying the still 1 may be a valved branch 43 connected by a tube 44 to the middle section 15, and, in order to draw off from the middle section 15, when desired, any excess of liquid at this point, said tube 44 may be connected by a valved tube 45 to the still 1.

Said lower section 38 may be adapted to be heated by means of a heater 46, which is connected by pipes 47 and 48 to said lower section 38, said heater 46 having pipes 49 and 59 for supplying steam thereto, while the pipe 48 may be provided with an expansion tank 51 which may be open at its upper end to the outer air by means of a cook 52. At its lower end, the lower section 38 may have a plate'53 in which the lower ends of the tubes 37 are secured, said plate 53 being connected to the lower section 38 and to a bottom 54 by means of e. g. bolts 55. The bottom 54 may have a window 56 to view the accumulation of liquid therein. From the lower end or weak alcohol receivers 61 and 62, which may be provided with valved compressed air pipes 63 and 64, respectively, to ,drivethe liquid therefrom by means of valved plpes 65 and 66, respectively, through a valved pipe 67 into a reservoir 68, which may be also 'cooled by a current of water supplied through an inlet pipe 71 and drawn off by an overflow pi e 72. The-condensatefrom the condenser 0 may pass through a coil condenser 7 3, preferably supplied with a current of cooling water entering by the pipe 72 and escaping by an overflow pipe 7 4, The high proof alcohol may be drawn oif from the coil 7 3 by a pipe 7 5, and may be thence conveyed into a tail box 76, from which it may be conveyed by valved pipes 77 and 78 to high-proof alcohol receivers 79 and 80, respectively. These receivers 79 and 80 may be, furthermore, provided respectively with valved pipes 81 and 82, which may be connected to a valve pipe 83, adapted to apply a vacuum to said receivers. The high proof alcohol from said receivers 79 and 80V may be discharged therefrom by means of valved pipes 84 and 85, respectively, and thence by a pipe 86 into the reservoir 68 and from said reservoir by means of a pipe 87 into the sup- P y an 9,

Any vapors which are not condensed in the tubular condenser may pass outwardly from the upper portion of the same by means of a pipe 88 to a suction tank 89, from which anycondensate that accumulates may be conveyed away to the supply tank 9 by means of a valved pipe 90. Said suction tank 89 may be, furthermore connected to the vacuum pipe 83 previously referred to and may be, furthermore, connected by a pipe 91 to a vacuum pump 92 of any desired it e.

linthe operation of my process, it will be understood that many different materials may be treated in the apparatus described, and that alcohols of many different kinds and strengths may be operated upon in accordance therewith.

For example, however, I may carry out the process by the treatment of an aqueous ethyl alcohol containing approximately 35% of alcohol.

In order to start the process, the alcohol may be charged into the still 1, or may be introduced initially into the supply tank 9, in any desired manner. Furthermore, the preheater 26 may be operated to heat the upper section 22 of the rectifier to the desired temperature, that is to say a temperature depending on the vacuum, but of about 2 C. 6

below the boiling temperature of absolute alcohol at that pressure, but as soon as this temperature has been attained and as soon as vapors are received from the still 1, it will be understood that the preheater 26 will be disconnected and the cooler 29 may be thrown into operation instead, so as to maintain said temperature substantially constant.

If it is desired to have the tubes 37 supplied with liquid from the beginning of the operation of the apparatus, a quantity of weak alcohol .may be su plied thereto by means of the pipe 43, an if at this or any subsequent time the amount of liquid accumulating above the plate 36 is greater'than the desired amount, this may be drawn of]? to a greater or less extent by means of the pipe 45 and returned to the still 1.

Under the conditions described the vacuum pump 92 is now operated so as to produce a vacuum of not less than 27 inches of mercury.

The alcohol vapors which pass out frbm the pipe 12 are discharged into the middle section 15 above the diaphragm 18, and are thence discharged downwardly through the openings 19 around the tube 20, so that in this way the alcohol vapors become evenly distributed within the middle section 15, so that they will be uniformly supplied through the tubes 20. Any condensate which may accumulate above the diaphragm 18 also passes downwardly through the openings 19 and is received by the plate 36. The alcohol vapors passing into the lower ends of the tubes 20 will have a. strength of approximately 82% alcohol. As these vapors pass upwardly in the tubes 20, a portionthereof will become condensed during the travel of the vapors through said tubes, so that by the time the vapors reach the upper ends of the tubes 20 there will be a descending film of condensed water and alcohol extending from the upper to the lower portion of said tubes 20.

Owing to the fact, however, that under the influence of a vacuum, solutions of alcohol in water, even when a proximating absolute alcohol, are in equi ibrium with the vapors evolved therefrom only when said vapors contain a larger percentage of alcohol than the liquid adjacent thereto, the ascending current of vapors in the tubes 20 will become enriched in alcohol by reason of the condensation therefrom of a liquid which the tubes 20 will be formed; from vapors richer in alcohol than the vapors in the lower ends of the tubes 20. Therefore, the tubes 20 contain an ascending current of alcohol vapors becoming increasin ly richer in alcohol as they ascend, while t e inner walls of said tubes will carry a descending film of aqueous alcohol becoming progressively poorer in alcohol.

Furthermore, because of the reverse directions in which these two currents flow, the vapors at any one point in the tubes 20 will be continually brought into contact with a portion of the film of liquid which is richer in alcohol than a bod of aqueous alcohol that would be in equi ibrium with the vapors at said point, so that there will result an interchange between the vapors at every point with the liquid with which it is in contact which will increase the percentage of alcohol in the vapors and decrease the percentage of alcohol in the liqu'id. In this way the increase in the percentage of the alcohol in the current of ascending vapors will become very much accelerated.

When, therefore, the vapors leave the upper ends of the tubes 20, they will be found to very closely approximate pure alcohol,

and may, for example, in the example of my invention described in detail herein be comprised of 99 or 99.5% alcohol.

Under the conditions described the condensate which leaves the lower ends of the tubes 20 falls downwardly in the middle section 15 upon the plate 36 and is there caused to form very thin films of liquid descending upon the inner walls of the tubes 37 by reason of the L-shaped pipes 40, which not only act to form said films, but, by reason of their shape, prevent the entry of drops'of liquid into said tubes. The liquid at this point will in the example of my invention described be comprised of approximately, 35% alcohol. As the films of liquid descend in the tubes 37, the heater 46 will cause a current of vapor to be formed therein, so that here again there will be an ascending current of alcohol and water vapors gradually becoming richer in alcohol by reason of their contact with the descending current of the liquid aqueous alcohol in substantially the same manner as described in connection with the operation of my invention within the upper section 22, which liquid becomes gradually poorer in alcohol until the liquid which passes out from the lower ends of the tubes 37'is comprised substantiall of pure Water.

The liquid which thus accumulates at the bottom of the rectifier 16 may be drawn off by the pipe 57 and received in the receivers 61 and 62, from which the same may be discharged by the pipe 69 or may be conducted into the reservoir 68. In case the liquid mamas thus recovered is weak alcohol, it will be conducted into the reservoir 68 for further treatment in accordance with my. invention, as by returning to the still 1; but in case it is comprised of substantially pure water, it will be drawn ofi' by the pipe 69 and discharged from the apparatus.

The vapors passing out through the upper ends of the tubes 40 become commingled with the vapors supplied from the still 1 and pass upwardly through the tubes 20 for treatment in the manner which has been described above.

The vapors which pass out from the upper end of the rectifier 16 and which maybe comprised, as previously indicated, of vapors having a strength of 99 or 99.5% alcohol pass into the tubular condenser 70, where they are condensed, and from this point pass into the coil condenser 73, from which the condensate is conveyed by ipe 75 into the alcohol receivers 79 and 80.

If it is desired at any time to redistill the alcohol contained in the receivers 79 and 80, as in the case where it would be desired to lncrease the strength thereof by redistillation, said alcohol may be conveyed by the pipe 86 into the reservoir 68, from which said alcohol may be forced by compressed air into the supply tank 9. Furthermore, any vapors which are not condensed in the tubular condenser and which may subsequently condense in the suction tank 89 may be conveyed to the supply tank 9 by means of the pipe 90. From this point the alcohol in the supply tank 9 may be conducted to the still 1 for redistillation, if desired.

During the distillation, the progress thereof may be determined by viewing the action of the same through the various windows, tail boxes, etc.

\Vhile I have described my invention above in detail, I wish it to be understood that many changes may be made therein without departing from the spirit of the invention. For example, by the term still I mean any vapor-supplying means.

claim:

l. A process of rectifying alcohol comprising distilling of aqueous alcohol, passing the vapors through long tubes maintained under a vacuum and at a. temperature below the boiling point of absolute alcohol corresponding to the low pressure used, and condensing the alcohol issuing from the tops of the tubes.

2'. A process of rectifying alcohol comprising distllling of aqueous alcohol, passing the vapors through long tubes maintained under a vacuum of not less than 27" mercury and at a temperature below the boiling point of absolute alcohol at the above pressure and condensing the alcohol issuing from the tops of the tubes.

3. A process of rectifying alcohol comprispressure and at a temperature slightly below the boiling point of absolute alcohol corresponding to the low pressure.

5. A process of removing water from alcoholic vapors comprising passing them through a long tube maintained under low pressure and at a temperature slightly beow the boiling point corresponding to the low pressure, and condensing the alcohol issuing from the top of the tube.-

6. A process of removing water from alcoholic vapors comprising passing them through a long tube maintained under low pressure and at a temperature slightly below the boiling point of absolute alcohol at that pressure, passing the liquid condensed into another inclined tube and evaporating alcohol therefrom and passing it into the first tube, and condensing the alcohol issuing from the first mentioned tube.

7. A process of removing water from alcoholic vapors comprising passing them through a rectifying column under a low pressure and maintaining the column at a temperature slightly below the boiling point of absolute, alcohol at that pressure.

8. A process of removing water from alcoholic vapors comprising passing them through a rectifying column under a low pressure and cooling the column to prevent boiling, and condensing liquid therein.

9. A process of removing water from an alcoholic liquid comprising distilling aqueous alcohol, passing the vapors through long tubes- While maintaining a vacuum therein, and a temperature slightly below the boiling point of absolute alcohol corresponding to the vacuum, said tubes being preheated before conducting the vapors therethrough, and condensing aqueous liquid from the vapors.

10. A process of removing water from alcoholic vapors comprising passing them through a rectifying column under low pressure and at a temperature about 2 below the boiling point of absolute alcohol at the corresponding pressure.

11. A process of removing water from alcoholic vapors comprising passing them through a rectifying column comprising of absolute alcohol long vertical tubes under low pressure, and cooling the tubes without condensing out all of the alcohol vapors passing therethrough.

12. A process of removing water from a1 coholic vapors comprising passing them through a rectifying column comprising long vertical tubes under low pressure, cooling the tubes without condensing out all of the alcohol vapors passing therethrough, and condensing the nearly pure alcohol vapor passing from the tops of the tubes.

13. A process of removing water from alcohol vapors comp-rising passing them through a tubular rectifying column under low pressure and cooling the column without condensing out all of the alcohol vapors passing therethrough.

14:- A process of rectifying alcohol comprising passing vapors of alcohol and water through a tubular rectifying column under low pressure, cooling the column so as to condense out non-alcoholic and partly alcoholic vapors passing therefrom, and condensing the practically pure alcohol vapor issuing from the top of the column.

15. A process of rectifying alcohol comprising distilling an aqueous alcohol, passing the vapors upwardly through long vertical tubes maintained under a vacuum and at a temperature slightly below the boiling point of absolute alcohol corresponding to the low pressure, condensing the nearly absolute alcohol issuing from the tops of the tubes, flowing the aqueous alcoholic liquid condensate in the said tubes down another set of tubes positioned below the former while maintaining the films of liquid under conditions of temperature and pressure similar to the above, passing the alcoholic vapors upwardly into the upper set of tubes and removing the weak alcoholic liquid from the bottom of the lower tubes.

16. The process which comprises distilling mixed vapors, passing them into a vapor distributor and thence into a tubular rectifier by feeding said vapors concentrically around the exteriors and into the ends of the tubes of the rectifier.

17. The process which comprises distilling mixed alcohol and Water vapors, passing them into a vapor distributor and thence into a tubular rectifier by feeding said vapors concentrically around the exteriors and into the ends of the tubes of the rectifier.

In testimony that I claim the foregoing 

